Sample supply device for automatic analysis apparatus



A. FERRARI May 24, 1966 SAMPLE SUPPLY DEVICE FOR AUTOMATIC ANALYSIS APPARATUS 3 Sheets-Sheet 1 Filed Dec. 24 1963 y 1966 A FERRARI 3,252,327

SAMPLE SUPPLY DEVICE FOR AUTOMATIC ANALYSIS APPARATUS Filed Dec. 24, 1963 :5 Sheets-Sheet 2 ATTORN EY May 24, 1966 FERRAR| 3,252,327

SAMPLE SUPPLY DEVICE FOR AUTOMATIC ANALYSIS APPARATUS Filed Dec. 24, 1963 5 Sheets-Sheet 5 Andras Fer/471' BY MES ATTORNEY m l .im

f i l Y j J J 36 V INVENTOR.

United States Patent 3,252,327 SAMPLE SUPPLY DEVBCE FOR AUTGMATIC ANALYSIS AlPARATUS Andres Ferrari, Scarsdale, N.Y., assignor to Technicon Instruments Corporation,.Chauncey, N.Y., a corporation of New York Filed Dec. 24, 1963, Ser. No. 333,023 3 Ciaims. (Cl. 73-423) This invention relates to automatic analysis apparatus and, more particularly, to sample supply means for such apparatus.

One object of the invention is to provide means for introducing air or other gas into the liquid samples in the receptacles during the sample take-off operation and also preferably immediately before the take-off operation whereby to stir the liquid and thereby prevent settling out in the receptacle of particulate matter suspended in the liquid.

Another object is to provide the sample supply device with means for supplying a wash liquid between successive samples.

Another object of the invention is to provide sample supply apparatus having a sample-liquid take-off tube or pipette in which provision is made for the introduction of air or other inert gas into the tube preferably near its sample inlet end for dividing the flowing stream of sample liquid into segment of the liquid spaced from each other by intervening segments of the inert gas, whereby insoluble particulate matter which may be present in the liquid which is to be analyzed is prevented from settling out during the flow of the liquid through the tubular conduits and other parts of the analysis apparatus.

A further object is to provide the sample supply device with means for automatically washing the air-introducing and sample-liquid take-01f tubes between sample take-01f operations.

The above and other objects, features and advantages of this invention will be apparent from the following description of the presently preferred embodiment of the invention considered in connection with the accompanying illustrative drawings.

In the drawings:

FIG. 1 is a top plan view of the sample supply device embodying the invention with the device connected to an analysis apparatus which is diagrammatically illustrated;

FIG. 2 is a perspective view, partly in section, of part of the sample supply device;

FIG. 3 is a sectional view taken on line 33 of FIG. 1.

FIG. 4 is a top plan view of part of the apparatus with parts omitted;

FIG. 5 is a sectional view, on a larger scale, on the line 55 of FIG. 1; and

FIG. -6 is a sectional view, on a larger scale, of the take-01f device with the associated air-introducing means.

Referring now to the drawings in detail, the sample supply device 10, briefly described, comprises a carrier here shown as a turntable 12 which is intermittently turned by suitable mechanism disposed within a housing 14, said mechanism being illustrated by FIGS. 2, 3 and 4 and hereinafter more particularly described. The turntable comprises a rack 16 which carries a series of removable tubes 18 which are receptacles for the liquid samples, said tubes being disposed laterally of each other in a circular row. For this purpose, rack 16 is provided with a series of holes 20 and the tubes have a flaring top 22 which rests on the marginal edge of the rack around the openings through which the cup projects, as shown by FIGS. 5 and 6.

A take-01f device 24 is mounted on the top of the housing 14 laterally of the rack 16 and laterally of a stationary receptacle 26 which provides a wash liquid for the liquid samples. The receptacle is mounted on top of the housing 14, laterally outwardly of the carrier 12. The take-off device is mounted for movement laterally to positions above the tubes 18 and the receptacle 26, respectively, and is also movable up and down in said positions into and out of the cups and receptacle, respectively, for withdrawing the samples and wash liquid. The device includes a tubular or sheath member 28 through which the take-off tube 30 extends for connection by tube 31 to the pump 32 (FIG. 1) of the analysis apparatus for aspiration of the sample liquid and wash liquid from the cup and receptacle, respectively, and it is to be noted that in the up or retracted position of the take-off device, the inlet end 36 of the take-off tube 30 is exposed to the air so that the takeoff device is operative to aspirate air in said retracted position because of the operation of pump 32, whereby a stream of longitudinally spaced liquid samples is formed wherein the liquid samples are separated from each other by intervening segments of the wash liquid disposed between a pair of air segments. The wash liquid segments are efiective to cleanse the walls of the tubular passages of the analysis apparatus and prevent contamination of a sample by a preceding sample and this cleansing action is an addition to the cleansing action provided by the intervening air segments.

As herein illustrated, the receptacle 26 for the wash liquid comprises a rectangular block of a suitable plastic material having a pair of open top chambers 38 and 40 interconnected to each other at their upper ends by a passage 42. Chamber 38 is provided with an inlet 44 which is adapted to be connected to a suitable source of wash liquid which may be supplied through a con duit 46 of the analysis apparatus 34 by the pump 32. Chamber 40 is provided with an outlet which may be connected to a conduit 56 of the analysis apparatus for pumping the wash liquid from the receptacle by the action of pump 32. Said outlet is larger than the inlet 44 so that excess wash liquid which overflows into chamber 40 from chamber 38 through passage 42 is readily discharged through the outlet at a faster rate than the flow of the wash liquid into the receptacle to prevent any overflow of wash liquid from the receptacle.

A similar wash liquid receptacle 52 is provided for the tube 53 (FIG. 5) which is associated with tube 28 and is movable therewith into and out of the sample receptacles 18 and into and out of said receptacle 52. Water is supplied to recepticle 52 by pump 32 through tube 46', and is pumped out of said receptacle through tube 52.

The function of tube 53 is to introduce air into the liquid in the tube 18 which is next to the tube which is at the take-off station at which time the take-ofi tube 30 is positioned in the tube at the sample take-off station for the take-ofl' operation. Air is supplied to member 28 of take-ofli device 24 and to tube 53 by tube 54 through which air is pumped by pump 32. Tube 54 is connected to takeofl member 28 by the branch tube 55 which is in communication with the interior of member 28 through top closure member 55. Air passes from member 28 into the liquid in tube 18 through a passage 57 which leads to an opening 57 in member 28. Said passage 57 is formed in the lower closure member 59. Take-off tube 30 is supported in member 28 by members 55 and 59, as clearly shown by FIG. 6. A second passage 59 is provided in closure member 59 and has an inlet connected to air supply tube 61, which extends into member 58, and an outlet 61 which communicates with take-off tube 30 through an opening 31' therein. Air is pumped through tube 61 by 'pump 32. 'through tube 30 than is pumped through tube 61 and that pump 32, the tube 61a of the latter being connected to tube 61. The air which is transmitted through passage 57 stirs the liquid in tube 18 while the air which is transmitted by way of passage 59' to tube 31 segments the liquid which is pumped from tube 18 and also segments the wash liquid when take-off member 28 is disposed in wash liquid receptacle 26.

As previously indicated, the rack 16 is rotated intermittently to present each tube 18 in succession to the take-off device 24 and during this rotary movement, the take-01f device is in a retracted position above the tube and is aspirating air through the take-off tube 30. When the sample tube is carried into position and is under the inlet end 36 of the take-off tube, rotation of rack 16 stops and the take-01f device is operated and moves downwardly so that the inlet end of the take-oflf tube is disposed in the liquid sample for withdrawing a portion of the sample therefrom. After a portion of the sample is withdrawn from the tube, the take-off device is operated and moves up into a retracted position with the inlet end exposed to the atmosphere so that air is again aspirated through said inlet. position laterally, pivoting in a counterclockwise direction as viewed in FIG. 1, to a position where the inlet end of the tube 30 is above and in alignment with chamber 38 of receptacle 26. The take-off device then moves downwardly to immerse the inlet end of the take-off tube in the wash liquid in chamber 38 for withdrawing a portion of the liquid therefrom. After said portion is withdrawn, the take-ofl? device moves upwardly into a retracted position and in said position .air is again aspirated through the take-off tube. The take-off device is then moved laterally, pivoting in a clockwise direction as viewed in FIG. 1, until the inlet end of the take-01f tube is positioned above the next tube which contains the next liquid sample and it will be understood that said tube had previously been moved into position during the time that the inlet tube was withdrawn from the preceding sample tube. Indexing movement of the plate 16 occurs when the takeon tube is withdrawn from the sample tubes 18. It will be noted that air is pumped into tubes 53 and 61 under pressure while fluid is pumped through take-01f tube 30' and tube 31 by the aspiration effect of the pump tube of It will be understood that more fluid is pumped the internal diameters of tubes 31 and 31b are sufiiciently large for this purpose.

The mechanism for providing the up and down ,and lateral movement of the take-off device will now be described with respect to FIGS. 2, 3 and 4. The member 28 and tube 53 are secured to a bracket 56a which is mounted on a vertical rod 56 which is movable vertically in a sleeve 58 mounted on the housing 14. A grooved wheel 60 is secured to the lower part of rod 56. An arm 62 is pivotally mounted at 64 to a support 66 and the arm is provided with a bifurcated end 68 which has a pair of pins 70 whose ends are disposed in the peripheral groove 72 of wheel 60. A tension spring 74, whose opposite ends are secured to the housing 14 and arm 62, respectively, biases said arm into an upward position and roller 76, carried by arm 72, is biased by the spring into engagement with the cam 78 so that rotation of said cam moves the take-01f device 24 vertically up and down in timed relation with the rotation of rack 16. I

Lateral pivotal movement of the take-01f device is provided by the cam 80 which engages a roller 82 that is secured to an arm 84. One of the ends of the arm is pivoted at 86 and the opposite end is provided with a longitudinal slot 88. A link 90 is secured at one of its ends to rod 56 and its opposite end is provided with a pin 92 which slides in slot 88 of arm 84, the latter being biased by a tension spring 94 so that roller 82 is biased into engagement with cam 80. Rotation of said cam results in the lateral back and forth movements of the take-off device 24 in timed relation to the intermittent rotation of rack The take-01f device is then moved in its retracted 16 and the vertical up and down movement of the takeoff device.

The mechanism for turning the turntable 12 is described in detail in the US. patent of Jack Isreeli, No. 3,038,340 issued June 12, 1962. As more fully described 'in said Isreeli patent, a Geneva gear 96 is mounted on a shaft 98 which is secured to a plate 100 of housing 14. A pinion gear 102 is mounted for rotation on shaft 98 and Geneva gear 96 is secured to the hub of said pinion gear. Gear 102 is in mesh with an intermediate gear 104 which drives a gear 106, the latter gear being secured to a drive shaft 108 on which the rack 16 is operatively mounted for intermittent rotation.

The driver for Geneva gear 96 is constituted by a pin 110 which projects upwardly from a gear 112 which is part of a speed change mechanism operated by the lever 114 shown in FIG. 4. An electric motor 116 turns a series of gears 117, which are mounted on the drive shaft of the motor and are part of the speed change mechanism, and drive gear 118 meshes with .gear 112 to drive pin 110 for operating the Geneva gear 96 for intermittently rotating rack 16.

The lateral pivotal movement and the up and down movements of the take-ofi. device are also eifected by the operation of the Geneva gear mechanism since gear 112 is in mesh with a gear 120 to which cams 78 and 80 are secured. Rotation of pin 110 and gear 112 results in the simultaneous rotation of gear 120 and the operation of cam 78 and 80 so that the operation of the take-off device is in timed relation with the intermittent rotation of rack 16 of the turntable.

The liquid supply device 10 is especially useful for providing a stream of liquid samples separated fromeach other by intervening segments of wash liquids disposed between a pair of air segments to an analysis apparatus 34 of the type shown and described in US. Patent No. 2,797,149 issued June 25, 1957. Briefly described, the apparatus includes the previously mentioned pump 32, which is a proportioning pump preferably of the type shown in US. Patent No. 2,935,028 issued May 3, 1960, a dialyzer (not shown), a colorimeter 124 and a recorder 126 which is operated under the control of the colorimeter. The sample liquid stream containing the intervening wash and air segments is transmitted from the take-01f device 24 through conduit 31 and air is introduced into the sample stream at opening 31' of take-off tube 30 to segmentize the liquid segments of the stream, as illustred in FIG. 6, the air segments AS being effective to cleanse the walls of the tubular passages of the apparatus as previously indicated and as described in the aforementioned patent. A processing liquid is transmitted through conduit 133 and is mixed with the liquid of the sample stream in a horizontal helical mixing coil (not shown) and is transmitted through the dialyzer, at one side of the membrane thereof. An air segmented recipient liquid stream is transmitted through the dialyzer at the other side of the membrane thereof and a dialyzate stream is formed which is transmitted from the dialyzer through a helical mixing coil 138 and then to the colorimeter 124 for colorimetric examination of the treated sample. The results of the examination are recorded on the recorder 126. The recipient stream may contain a color producing agent and is transmitted through conduit 140 while the segmentizing air is transmitted through conduit 142. The air segments in the dialyzate stream are removed from the stream by the vented tube 144 prior to colorimetric examination. The undiftused portions of the sample segmentedstream are discharged from the dialyzer through an outlet at the first mentioned side of the dialyzer membrane. a

While I have shown and described the preferred embodiment of the invention, it will be understood that the invention may be embodied otherwise than as herein specifically illustrated or described, and that certain changes in the form and arrangement of parts and in the specific manner of practicing the invention may be made without departing from the underlying idea or principles of this invention within the scope of the appended claims.

What is claimed is:

1. Liquid-sample supply apparatus, comprising: a carrier for a plurality of liquid sample containers; sheath means; means for sequentially inserting said sheath means into each of said containers; said sheath means having a first passageway therethrough having an outlet coupled to a suction means and an inlet adapted to pass thereinto liquid from the container into which said sheath means is inserted, a second passageway having .an inlet coupled to a source of gas and an outlet merging into said first passageway downstream of said inlet of said first passageway and adapted to pass gas thereinto, and a third passageway having an inlet coupled to a source of gas and an outlet adapted to pass gas into the liquid of the container into which said sheath means in inserted.

2. Liquid-sample supply apparatus, comprising: a carrier for a plurality of liquid sample containers; sheath means; means for sequentially inserting said sheath means into each of said containers; said sheath means having a first passageway therethrough having an upper outlet coupled to a suction means and a lower, downwardly directed inlet adapted to pass thereinto liquid from the container into which said sheath means is inserted; a second passageway having an upper inlet coupled to a source of gas and a lower outlet merging into said first passageway downstream of said inlet of said first passageway and adapted to pass gas thereinto; and a third passageway having an upper inlet coupled to a source of gas and a lower, laterally directed outlet adapted to pass gas into the liquid of the container into which said sheath means is inserted.

3. Liquid-sample supply apparatus, comprising: a carrier for a plurality of liquid sample containers; sheath means; means for sequentially inserting said sheath means into each of said containers; said sheath means comprising an outer tube; an upper plug closing the upper end of said outer tube; a lower plug closing the lower end of said tube; an inner second tube passing axially through a bore in said upper plug, said outer tube and a bore in said lower plug, the upper end of said second tube serving as an outlet and coupled to a suction means, the lower end of said second tube serving as an inlet and adapted to pass thereinto liquid from the container into which said sheath means is inserted; an additional bore in said upper plug having an upper laterally directed por-' *tion serving as an inlet and coup-led to a source of gas and a lower axially directed portion communicating with the interior of said outer tube, an additional bore in said lower plug having an upper axially directed portion communicating with the interior of said outer tube, and a lower laterally directed portion serving as an outlet and aligned with an aperture in the side wall of said outer tube to pass gas into the liquid of the container into which said sheath means is inserted; said additional bore in said upper plug having an additional upper axially directed portion communicating with said first mentioned lower axially directed portion, an inner third tube having an upper end coupled to a source of gas and passing through said upper and lower axially directed portions of said additional bore in said upper plug, a further additional bore in said lower plug having an upper axially directed portion connected to the lower end of said inner third tube and a lower laterally directed portion serving as an outlet and aligned with an aperture in the side wall of said inner second tube and adapted to pass gas into said second inner tube downstream of said inlet of said second inner tube.

References Cited by the Examiner UNITED STATES PATENTS 638,046 11/1899 Dobson 26l12l 3,107,537 10/1963 Isreeli et a1. 73-423 3,134,263 5/1964- De Iong 73423 3,186,235 6/1965 Ferrari 73-423 LOUIS R. PRINCE, Primary Examiner.

S. C. SWISHER, Assistant Examiner. 

1. LIQUID-SAMPLE SUPPLY APPARATUS, COMPRISING: A CARRIER FOR A PLURALITY OF LIQUID SAMPLE CONTAINERS; SHEATH MEANS; MEANS FOR SEQUENTIALLY INSERTING SAID SHEATH MEANS INTO EACH OF SAID CONTAINERS; SAID SHEATH MEANS HAVING A FIRST PASSAGEWAY THERETHROUGH HAVING AN OUTLET COUPLED TO A SUCTION MEANS AND AN INLET ADAPTED TO PASS THEREINTO LIQUID FROM THE CONTAINER INTO WHICH SAID SHEATH MEANS IS INSERTED, A SECOND PASSAGEWAY HAVING AN INLET COUPLED TO A SOURCE OF GAS AND AN OUTLET MERGING INTO SAID FIRST PASSAGEWAY DOWNSTREAM OF SAID INLET OF SAID FIRST PASSAGEWAY AND ADAPTED TO PASS GAS THEREINTO, AND A THIRD PASSAGEWAY HAVING AN INLET COUPLED TO A SOURCE OF GAS AND AN OUTLET ADAPTED TO PASS INTO THE LIQUID OF THE CONTAINER INTO WHICH SAID SHEATH MEANS IS INSERTED. 